Abstract
Tungsten permanent modifier with coinjection of Pd(NO3)2 and W–Ru permanent modifiers are proposed for the direct and simultaneous determination of As, Bi, Pb, Sb, and Se (group 1) and Co, Cr, Cu, Fe, and Mn (group 2), respectively, in milk by graphite furnace atomic absorption spectrometry. The performance of modifiers was evaluated by means of thermal behavior of analytes, sensitivity, atomic signal profile, repeatability, graphite tube lifetime, and background intensity. An air-assisted pyrolysis step was necessary to quantitative elimination of the organic matter. After methods optimization, 14 commercial milk samples were analyzed. The found concentrations of As, Bi, Pb, Sb, Se, Co, and Cr were lower than their limit of detection (2.13, 2.21, 1.49, 1.63, 2.05, 1.0, and 1.2 μg L−1, respectively). Concentrations of Cu, Fe, and Mn were in the 1.58–5.74 μg L−1, 9.79–49.3 μg L−1, and 2.25–4.08 μg L−1 intervals, respectively. The limits of detection for Cu, Fe, and Mn were 1.7, 5.3, and 2.0 μg L−1, respectively. The accuracy of methods was checked after analysis of two milk standard materials. Results for Cr, Cu, Fe, Mn, Pb, and Mn were in agreement with certified values of SRMs at the 95% confidence level. Accuracy was also evaluated by addition–recovery tests and recoveries in the 86–127% range were obtained for all elements. The use of pretreat platform of graphite tubes with W or W–Ru allowed enlarging the lifetime of atomizer in 750 heating cycles.
Similar content being viewed by others
References
Campillo N, Viñas P, López-García I, Hernández-Córdoba M (2000) Determination of arsenic in biological fluids by electrothermal atomic absorption spectrometry. Analyst 125:313–316
Correia PRM, Oliveira E, Oliveira PV (2002) Simultaneous determination of manganese and selenium in serum by electrothermal atomic absorption spectrometry. Talanta 57:527–535
Correia PRM, Oliveira PV, Neto JAG, Nóbrega JA (2004) Silver as internal standard for simultaneous determination of Cd and Pb in whole blood by electrothermal atomic absorption spectrometry. J Anal At Spectrom 19:917–922
Currie LA (1999) Nomenclature in evaluation of analytical methods including detection and quantification capabilities (IUPAC Recommendations 1995). Anal Chim Acta 39:105–126
Freschi GPG, Freschi CD, Oliveira SR, Neto JAG (2006) Evaluation of Ir-based modifiers in the simultaneous determination of As, Bi, Pb, Sb, and Se in milk by graphite furnace atomic absorption spectrometry. Atom Spectros 27:179–185
Freschi GPG, Freschi CD, Neto JAG (2008) Evaluation of different rhodium modifiers and coatings on the simultaneous determination of As, Bi, Pb, Sb, Se and of Co, Cr, Cu, Fe Mn in milk by electrothermal atomic absorption spectrometry. Microchim Acta 161:129–135
García JCR, García JB, Latorre CH, Martín SG, Crecente RMP (2005) Comparison of palladium–magnesium nitrate and ammonium dihydrogenphosphate modifiers for lead determination in honey by electrothermal atomic absorption spectrometry. Food Chem 91:435–439
Harnly JM, Radziuk B (1995) Effect of furnace atomization temperatures on simultaneous multielement atomic absorption measurement using a transversely heated graphite atomizer. J Anal At Spectrom 10:197–206
Kopysc E, Bulska E, Wennrich R (2003) On the use of noble metals modifiers for simultaneous determination of As Sb and Se by electrothermal atomic absorption spectrometry. Spectrochim Acta B Atom Spectros 58:1515–1523
Lima EC, Brasil JL, Santos AHDP (2004) Determination of antimony in environmental samples by ETAAS using different permanent modifier. Microchim Acta 146:21–29
Luna AS, Campos RC (1999) Determination of Mn in whole blood and urine by graphite furnace AAS using different modifiers. Atom Spectros 20:108–112
Nomura CS, Correia PRM, Oliveira PV, Oliveira E (2004) W+Rh as permanent chemical modifier in simultaneous atomic absorption spectrometry: interference studies on As, Cd, Pb and Se determination. J Braz Chem Soc 15:75–82
Ortner HM, Bulska E, Rohr U, Schlemmer G, Weinbruch S, Welz B (2002) Modifiers and coatings in graphite furnace atomic absorption spectrometry—mechanisms of action (a tutorial review). Spectrochim Acta B Atom Spectros 57:1835–1853
Pereira LA, Amorim IG, Silva JBB (2006) Determination of cadmium, chromium and lead in marine sediment slurry samples by electrothermal atomic absorption spectrometry using permanent modifiers. Talanta 68:771–775
Rademeyer CJ, Radziuk B, Romanova N, Skaugset NP, Skogstad A, Thomassen Y (1995) Permanent iridium modifier for electrothermal atomic absorption spectrometry. J Anal At Spectrom 10:739–745
Soylak M, Tuzen M, Narin I, Sari H (2004) Comparison of microwave dry and wet digestion procedures for the determination of trace metal contents in spice samples produced in Turkey. J Food Drug Anal 12:254–258
Soylak M, Saracoglu S, Tuzen M, Mendil D (2005) Determination of trace metals in mushroom samples from Kayseri, Turkey. Food Chem 92:649–652
Volynsky AB (2004) Comparative efficacy of platinum group metal modifiers in electrothermal atomic absorption spectrometry. Spectrochim Acta B Atom Spectros 59:1799–1821
Volynsky AB, Wennrich R (2001) Comparative efficiency of Pd, Rh and Ru modifiers in electrothermal atomic absorption spectrometry for the simultaneous determination of As, Se and In in a sodium sulfate matrix. J Anal At Spectrom 16:179–187
Welz B, Schlemmer G, Mudakavi JR (1992) Palladium nitrate–magnesium nitrate modifier for electrothermal atomic absorption spectrometry. Part 5. Performance for the determination of 21 elements. J Anal At Spectrom 7:1257–1271
Zanão RA, Barbosa F Jr, Krug FJ, Abdalla AL (2002) Direct determination of selenium in whole blood by ETAAS using W–Rh-coated platform and co-injection of Rh as thermal stabilizer. Spectrochim Acta B Atom Spectros 57:291–301
Zhang L, Morita Y, Yoshikawa K, Isozaki A (2007) Direct simultaneous determination for ultratrace As, Se and Sb in river water with graphite-furnace atomic absorpion spectrometry by TiO2-slurry sampling. Anal Sci 23:365–369
Acknowledgments
The authors would like to thank the Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP) for financially supporting this work, the Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq) for researchships to JAGN, and the Coordenadoria de Aperfeiçoamento de Pessol de Ensino Superior for fellowships to GPGF and CDF.
Author information
Authors and Affiliations
Corresponding author
Rights and permissions
About this article
Cite this article
Freschi, G.P.G., Fortunato, F.M., Freschi, C.D. et al. Simultaneous and Direct Determination of As, Bi, Pb, Sb, and Se and Co, Cr, Cu, Fe, and Mn in Milk by Electrothermal Atomic Absorption Spectrometry. Food Anal. Methods 5, 861–866 (2012). https://doi.org/10.1007/s12161-011-9323-0
Received:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s12161-011-9323-0